CN103219065B - A kind of environmental-friendly conductive sizing agent based on carbon nanotube-nano copper powder - Google Patents
A kind of environmental-friendly conductive sizing agent based on carbon nanotube-nano copper powder Download PDFInfo
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Abstract
A kind of environmental-friendly conductive sizing agent based on carbon nanotube-nano copper powder, be made up of surface treated nano copper particle, carbon nano-tube, additive and organic solvent through carbon nano tube dispersion liquid process, described surface treated nano copper particle surface band negative electrical charge and average grain diameter is 50-150nm, the mass percent of each component is: surface treated nano copper particle 10-20wt%, additive 1-10wt%, organic solvent 10-20wt%, through the carbon nano-tube of carbon nano tube dispersion liquid process be surplus.In advantage of the present invention be: this electrocondution slurry has the double dominant of carbon nano-tube and precious metal material concurrently, carbon nano-tube has good dispersive property in the slurry, there will not be sedimentation phenomenon, and slurry conducts electricity very well; The electrocondution slurry recipe ingredient used of preparation is all environment friendly and pollution-free.
Description
Technical field
The present invention relates to technical field of electronic materials, be specifically related to a kind of environmental-friendly conductive sizing agent based on carbon nanotube-nano copper powder.
Technical background
Along with electronics and information industry enters the stage of high speed development, electric slurry industry is also allowed to have had tremendous development.Electric slurry integrates metallurgy, chemical industry, electronic technology, is a kind of electronic functional material with high-tech, therefore, has the status that can not be substituted in electron trade.Silver powder and electric slurry series of products thereof are that the while of being most widely used in electronics industry, consumption is also maximum a kind of noble metal powder, the basic function material producing various electronic component products, mainly for the manufacture of integrated circuit, capacitor, MLCC, electrode of solar battery, radio frequency identifiable design label etc.Along with the increase of demand and kind, people for the development of electrocondution slurry also in continuous progress, various new-type electrocondution slurry emerges in an endless stream, wherein especially popular with copper slurry, be because its production cost is lower than silver slurry on the one hand, on the other hand, although slightly inferior and silver paste in conductivity, but people are still more ready to select copper slurry, and therefore, the research being directed to conductive copper paste in recent years emerges in an endless stream.But these slurry major parts take all Metal Phase as main conductive function phase, in the majority especially especially with metal dusts such as silver powder, copper powder, nickel powders.Mention in patent CN101593568 and add carbon nano-tube in electrocondution slurry, and become a part for conductive phase, and for its existence form and how to process and not mentioned and slurry not environmentally.
Summary of the invention
The object of the invention is for above-mentioned existing problems, provide a kind of environmental-friendly conductive sizing agent based on carbon nanotube-nano copper powder, this electrocondution slurry has good electric conductivity and environmental protection.
Technical scheme of the present invention:
A kind of environmental-friendly conductive sizing agent based on carbon nanotube-nano copper powder, be made up of surface treated nano copper particle, carbon nano-tube, additive and organic solvent through carbon nano tube dispersion liquid process, described surface treated nano copper particle surface band negative electrical charge and average grain diameter is 50-150nm, the mass percent of each component is: surface treated nano copper particle 10-20wt%, additive 1-10wt%, organic solvent 10-20wt%, through the carbon nano-tube of carbon nano tube dispersion liquid process be surplus.
Described carbon nano-tube is the mixture of one or both arbitrary proportions in Single Walled Carbon Nanotube and multi-walled carbon nano-tubes.
Described carbon nano tube dispersion liquid is surface-active ion liquid, is specially dodecyl-3-methylimidazole bromine (C12mimBr) or myristyl-3-methylimidazole bromine (C14mimBr).
Described additive is binding agent and thickener and levelling agent, wherein binding agent is epoxy powder coating, thickener and levelling agent are the rheology modified thickener of polyurethane or hydrophobically-modified alkali swelling type thickener, and the mass ratio of binding agent and thickener and levelling agent is 1:1.
Described organic solvent is the mixture of one or both arbitrary proportions in ethyleneglycol monophenylether and ethylene glycol phenyl ether acetate.
A described preparation method based on the environmental-friendly conductive sizing agent of carbon nanotube-nano copper powder, step is as follows:
1) with chemical reduction method, mantoquita is reduced, prepare the nano copper particle that particle diameter is 50-150nm, and negative electrical charge on the nano copper particle surface band making preparation;
2) prepare the carbon nano-tube of surface with positive charge with surface-active ion liquid, then evenly spread in organic solvent;
3) add in the organic solvent containing carbon nano-tube by the nano copper particle processed and other additives, ultrasonic extremely each component mixes and can obtain electrocondution slurry.
A kind of described application based on the environmental-friendly conductive sizing agent of carbon nanotube-nano copper powder, can be used for electrode of solar battery, chip multilayer ceramic capacitor (MLCC), also can be used in the distribution type of the encapsulation of meticulous line pattern and multiple micro element, connection and wiring board.
Technical Analysis of the present invention:
1) nano copper particle why will on surface treatment band negative electrical charge, being to allow copper powder can be adsorbed on carbon nano tube surface better, giving full play to the advantage that carbon nano-tube and noble metal combine.
2) addition of nano copper particle is little, not it can be used as main conductive function phase, but in order to auxiliary carbon nano-tube, make the carbon nano-tube having copper powder with metallic character, and too much consumption copper powder can by treated carbon nano tube surface with positive charge all neutralize, cause the dispersiveness of carbon nano-tube to decline, mutually tangle or sedimentation, thus the stability of electrocondution slurry is declined.Therefore, only use marginally copper powder, the booster action to carbon nano-tube can be played, the dispersiveness that carbon nano-tube is excellent can be ensured again.
3) epoxy resin of binder powdery paints is in sintering process, just can solidify being no more than at the temperature of 200 DEG C, can play in other slurries the effect added institute's resin and play as binding agent equally.
4) the present invention does not adopt traditional process for dispersing for carbon nano-tube, as added the dispersiveness that macromolecular compound etc. makes carbon nano-tube reach good, and adopt surface-active ion liquid to disperse carbon nano-tube, and use it in electrocondution slurry simultaneously, be the combination of a kind of ionic liquid and electrocondution slurry, and also rare report is combined for both.
In advantage of the present invention be: after a small amount of copper powder of the carbon nanotube adsorption in this electrocondution slurry, on the basis that improve electric conductivity, still can be scattered in slurry preferably and sedimentation phenomenon not occur.And selected epoxy powder coating binding agent can show good electric property after hardening.In the carbon nano tube compound material of this slurry, all material not only comprising carbon nano-tube can play respective performance, and overall performance also increases.In sintering process, the copper powder being adsorbed on carbon nano tube surface can become sheet by graininess, and what formed carbon nanotube portion is coated, and also can be connected to some extent between sheet with sheet, is more conducive to the formation of conductive network.The all compositions of this electrocondution slurry are ep-type material, are conducive to environmental protection.
Embodiment
Embodiment 1-4:
A described preparation method based on the environmental-friendly conductive sizing agent of carbon nanotube-nano copper powder, step is as follows:
1) with chemical reduction method, mantoquita is reduced, prepare the nano copper particle that particle diameter is 50-150nm, and negative electrical charge on the nano copper particle surface band making preparation;
2) prepare the carbon nano-tube of surface with positive charge with surface-active ion liquid, then evenly spread in organic solvent;
3) add in the organic solvent containing carbon nano-tube by the nano copper particle processed and other additives, ultrasonic extremely each component mixes and can obtain electrocondution slurry.
Electrocondution slurry spin-coating film on equal glass substrate prepared by embodiment, after sintering 45min, obtains conductive layer, and measure its resistivity at 300 DEG C.In embodiment 1-4, each amounts of components and conducting performance test the results are shown in Table 1.
Table 1
Testing result shows: this electrocondution slurry has good electric conductivity and environmental protection.
The electrocondution slurry of preparation can be used for electrode of solar battery, chip multilayer ceramic capacitor (MLCC), also can be used in the distribution type of the encapsulation of meticulous line pattern and multiple micro element, connection and wiring board.
Claims (5)
1. the environmental-friendly conductive sizing agent based on carbon nanotube-nano copper powder, it is characterized in that: by surface treated nano copper particle, the carbon nano-tube of surface with positive charge is prepared with surface-active ion liquid, additive and organic solvent composition, described surface treated nano copper particle surface band negative electrical charge and average grain diameter is 50-150nm, the mass percent of each component is: surface treated nano copper particle 10-20wt%, additive 1-10wt%, organic solvent 10-20wt%, preparing the surperficial carbon nano-tube with positive charge with surface-active ion liquid is surplus.
2. according to claim 1 based on the environmental-friendly conductive sizing agent of carbon nanotube-nano copper powder, it is characterized in that: described carbon nano-tube is the mixture of one or both arbitrary proportions in Single Walled Carbon Nanotube and multi-walled carbon nano-tubes.
3. according to claim 1 based on the environmental-friendly conductive sizing agent of carbon nanotube-nano copper powder, it is characterized in that: described surface-active ion liquid is specially dodecyl-3-methylimidazole bromine (C12mimBr) or myristyl-3-methylimidazole bromine (C14mimBr).
4. according to claim 1 based on the environmental-friendly conductive sizing agent of carbon nanotube-nano copper powder, it is characterized in that: described additive is binding agent and thickener-levelling agent, wherein binding agent is epoxy powder coating, thickener-levelling agent is the rheology modified thickener of polyurethane or hydrophobically-modified alkali swelling type thickener, and the mass ratio of binding agent and thickener-levelling agent is 1:1.
5. according to claim 1 based on the environmental-friendly conductive sizing agent of carbon nanotube-nano copper powder, it is characterized in that: described organic solvent is the mixture of one or both arbitrary proportions in ethyleneglycol monophenylether and ethylene glycol phenyl ether acetate.
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| CN106752804B (en) * | 2017-01-25 | 2019-04-09 | 山东凯盛新材料股份有限公司 | High temperature resistant, antistatic polyether ketone ketone powdery paints and preparation method thereof |
| CN108628502B (en) * | 2018-04-12 | 2021-07-06 | 重庆市中光电显示技术有限公司 | Water-based composite conductive slurry for touch screen and preparation method and application thereof |
| JP6526888B1 (en) * | 2018-08-01 | 2019-06-05 | Ｊｘ金属株式会社 | Laminate of ceramic layer and sintered body of copper powder paste |
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| CN101593568A (en) * | 2008-05-30 | 2009-12-02 | 三星电机株式会社 | The electrocondution slurry and the printed circuit board (PCB) that uses it that contain carbon nano-tube |
| EP2174910A1 (en) * | 2008-10-09 | 2010-04-14 | Exaenc Corp. | High conductive paste composite and method of producting the same |
| CN101864015A (en) * | 2010-06-25 | 2010-10-20 | 东华大学 | Method for preparing polyacrylonitrile/carbon nano tube composite material by taking ionic liquid as solvent |
| CN102198510A (en) * | 2011-04-27 | 2011-09-28 | 黑龙江大学 | Method for preparing nano copper/carbon nano tube composite powder by liquid phase method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100506439C (en) * | 2005-09-29 | 2009-07-01 | 江苏大学 | Method for preparing nanometer copper |
| CN102993820A (en) * | 2012-03-28 | 2013-03-27 | 杨阳 | Carbon nano material/metal nano material composite nano ink |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101593568A (en) * | 2008-05-30 | 2009-12-02 | 三星电机株式会社 | The electrocondution slurry and the printed circuit board (PCB) that uses it that contain carbon nano-tube |
| EP2174910A1 (en) * | 2008-10-09 | 2010-04-14 | Exaenc Corp. | High conductive paste composite and method of producting the same |
| CN101864015A (en) * | 2010-06-25 | 2010-10-20 | 东华大学 | Method for preparing polyacrylonitrile/carbon nano tube composite material by taking ionic liquid as solvent |
| CN102198510A (en) * | 2011-04-27 | 2011-09-28 | 黑龙江大学 | Method for preparing nano copper/carbon nano tube composite powder by liquid phase method |
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